Acetic Acid → 3-Chloro-1,1-diphenylpropene

HRID 1597728

반응식

HRID 1597728 반응식
[C:1]1([C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[CH2:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:15](O)(=O)C.C=O.[ClH:21]>O>[C:1]1([C:7]([C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)=[CH:8][CH2:15][Cl:21])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 313Hydrochloric Acid2회HCID 712FormaldehydeHCID 107401,1-Diphenylethylene

생성물 1

HCID 128901653-Chloro-1,1-diphenylpropene수율 99.7%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
30 °C

실험 절차

A 300-ml reaction flask was charged with 54.13 g (0.3 mol) of 1,1-diphenylethylene (9a), 108.26 g of acetic acid and 13.51 g (0.45 mol) of paraformaldehyde, and 13.67 g (0.375 mol) of hydrogen chloride was blown in with stirring at 30° C. for 3.5 hours. The reaction temperature was kept at 30° C. by cooling because of weak heat development. The blowing-in of hydrogen chloride was stopped, and the solution was stirred at the same temperature for 2 hours, followed by standing overnight. The reaction solution was poured into 200 ml of water, followed by extraction with 200 ml of toluene. The resulting product was washed with water, washed with 2% soda ash, washed with water, dried over magnesium sulfate, and concentrated to obtain 68.42 g of a crude chloride. It was distilled in a Claisen flask equipped with a vigreux to obtain 57.51 g.

후처리

  1. customA 300-ml reaction flask
  2. customwas kept at 30° C.
  3. temperatureby cooling because of weak heat development
  4. stirringthe solution was stirred at the same temperature for 2 hours
  5. waitby standing overnight
  6. extractionfollowed by extraction with 200 ml of toluene
  7. washThe resulting product was washed with water
  8. washwashed with 2% soda ash
  9. washwashed with water
  10. dry with materialdried over magnesium sulfate
  11. concentrationconcentrated

출처 및 근거

ORD 기록
ord-e4bf6426c0624bda8eb6dcad9ef3b14b
출처 데이터셋
uspto-grants-1998_04
특허 번호
US05736284

연결된 노트

불러오는 중…